Process of making a water resistant adhesive and to the product thereof



106. couPosmoms,

comma R PLAsnt Patented July 7, 1931- Examiner PATIENT; OFFICE i HARRY P. BANKS, OI SEATTLE, WASHINGTON rnocnss or MAKmG A WATER nnsrsraur ADHESIVE aun To run rnonuo'r iH'EBEOF No Drawing.

My invention relates to the process of making a. water resistant adhesive and the product thereof. More particularly, my in-' vention relates to the addition of a chemical 5 compound, namely furfural, to an adhesive, the base of which a esive is an olea inous Application filed January as, 1929. Serial No. 335,397. v 54 0 resistance of the same a e'sives manufactured without the addition of furfural.

have also discovered the same fact relative to adhesives embodying a mixture of oleaginous seed flours and casein. 55

For example, by way of comparison, in the seed flour which chemical compound lias the manufacture of adhesives for plywood I may efiect of increasing the dry strength of the resultant adhesive. Moreover, my invention relates to the increasing of the water resistance of said adhesive by the addition ofisaid furfural.

By oleaginous seeds I mean such oil bear ing seeds as so a beans, peanuts, cottonseed linseed. sesame seed, castor eans sunflower see e By olea inous seed flours I mean the products 0 tained by fine grinding of the residues remaining in the form of cake or meal after removal of the natural 01 conen 0 o eaginous see s in w o e oi in part, such removal being accomplished by pressure or extraction with solvents or acombination of both methods. And also I include in the 5 term oleaginous seed flour the flour obtained by fine grinding the material of hi h rotein content obtained by extraction 0 suc o eaglnous seed residues.

Wherever the term casein is used herein, so it is used to include roteln of milk whether such protein is in tlie form of wetcurd or dried and ground, and also whether sulphuric acid or hydrochloric acid precipitated or natural sour casein. y e erm ispersed condition, as ap-' lied to oleaginous seed flours and to casein,

, mean the state attained in thetransformation of a mealy or granular massto a more or less smooth mass in the presence of a liquid, 40 and to such extent as I thus refer to the deree of subdivision of particles I believe that vi am using the term dispersion not inconsistently with the accepted usage of colloid chemists. I have discovered that when furfural is used-in the manufacture or compounding o adhesives embodying oleaginous seed flours in dispersed condition the strength andwater resistance of the resultant adhesives are of greatly increased over the strength and water '11 illustrate 'with formulae embodying soya bean flour.

, (A) In a suitable mixing device place 500 1 parts of watgg. Stir in a dry mixture composed of 180 parts so a bean flour 28 parts calcium l1 drate,28 pa fis powdered rosin 40 parts ma nesium oxide. Add 30 pa% of 18% caustic soda solution and stir well. Add parts 0 water with 90 parts of a solution containim approximately 34% dry sodium silicate. tir 15 minutes and add 230 par ts of water and stir until smooth. Adhesitde (A) is now ready to be spread on plywoo v (B) Proceed exactly as in (A) except that 10 parts of technical grade fiirfural are added with the final addition of water.

Adhesives (A) and (B) were used to make 5 up 3-ply fir panels. These panels were storedfive days and test pieces cut from them to determine dry tensile strength in standard plywood testing machine.- Also test pieces were placed to soak in water for 48 hours and then tested on the same machine. Following are results in pounds per square inch;

' Aftasoaklng48houn Pound: Paul: A 175 50 B. 250 100 The marked increase in adhesive strength and water resistance of adhesive (B) over adhesive (A) is readily apparent.

Marked benefits were noted in similar formulae when the furfural was added at other stages of the compounding of the adhesive, y

f as for instance the furfural may be'mixed with the dry ingredients at time of adding same to the initlal'water in the mixing device. Furthermore, beneficial results were noted when oleaginou seed flour adhesives 10c embodying furfural were used on other woods such as pine, birch and gum.

:I have used an adhesive embodying the following ingredients in the proportions noted.

This adhesive (C) gave results of 225 lbs. per square inch dry strength, 120 lbs. per square inch strength after soaking for 48 hours, as compared with results of adhesive (A) above.

In further illustration of the marked effect of the use of furfural in adhesives embodying oleaginous seed flour I may give the following formula with results obtained with and without the use of furfural when the adhesive was appliedi'o both fir and birch ply- .wood.

I do not restrict myself to the ingredients or percentages of ingredients given in the formulae herein set forth, and particularlynot to the kind of oleaginous seed flour nor to the percentage of same, since these formulae are merely examples of a large number which I have used successfully and they are given herein for the purpose of illustration only.

same manner as adhesive (D) except that five parts of furfural are added with the final water.

Fir and birch veneer was laid up with ad sives are given below in pounds per square inch.

Dry tests l ig ifdu l i an Birch Fir' Birch veneer veneer veneer veneer Pounds Pounds Pounda Pounds Adhes ve (D) 195 2 20 Y 100 90 Adhesive (IE) 250 270 200 120 It will be observed that the addition of the strength and water resistance of the adhesive. As a further example of the benefit to be derived by the use of furfural in oleaginous seed flour adhesives I give the following:

, Parts (F) Soya bean flour 300 Calcium hydrate 54;

* Sodium carbonate -l- 30 Sodium fluoride 22 These ingredients were thoroughly mixed in the dry state, then 640 parts of water were placed in a suitable mixing device, the above furfural has very markedly increased the Sova bean flour 72.5% miXtuF'e of dry ingredients added and thor- Calcium hydrate 12.3% ug y filrred, then 452 parts" of water were Rosin (pdwdered) 3.9% added and the Whole stirred until free from Pot i permanganate 03% lumps. The adhesive is now ready for use Sodium fluoride 11.0% [and y be deslgnated 2 adhesive These ingredients are thoroughly mixed in the dry state in the following manner: 1000 parts of soya bean flour, 15-0 parts of calcium hydrate, 225 parts of rosin, 20 parts of potassium permanganate, are 'mixed together dry, sacked off and allowed to stand for aging urposes for a period of thirty days or onger; Then, 351% parts of this preliminary dry mix,.800 parts of soya bean fiour, parts of calcium hydrate, 158 parts of sodium fluoride: are mixed together dry and sacked off and this mixture comprises the percentage formula given above.

Then 250 lbs. of water are placed in a mechanical mixer of suitable type. One hundred-pounds (100 lbs.) ofthe'above described mixture of dry ingredients are added to the water and the whole stirred well. Then 75 lbs. of water are added and the whole stirred until smooth and free from lumps.

The adhesive is now ready .lUl. se on the material to be glued, such for instance as ply- \(?V](5())d, and may be designated as adhesive Adhesive (E) is prepared exactly in the ;(G) Adhesive (G) was prepared exactly the same as adhesive (F) except that ten '1 parts of furfural were added with the'final water. p

Adhesives (F) and (G) were spread on fir plywood, aged' and tested dry; soaked in water for 48 hours and tested as described for preceding experiments with the following results: Tests alter Dry tests soaking 48 hours lou'nds per 'Pau'nda per, square inch square inch' Adhesive (F) 215 115 Adhesive (G) 245 These tests show an increase of approximately fourteen per "cent (14%) in dry strength and approximately twenty-seven percent (27%) in wet adhesive strength as thedirect result of the use of furfural.

Again for purposes of illustration I give below several formulae which I have used in which one of the ingredients is furfural. The results obtained with adhesives made with O a a... 106. COMPOSITIONS, tress COAllNG R PLASTIC these formulae all show improvement over results obtained with similar formulae from which the furfural was omitted.

Parts (H Peanut flour 180 5 Calcium hydrate 28 Powdered rosin a 28 18% Caustic soda solution 3O In further exemplification of the scope of my invention I may cite examples of the in creased strength developed in adhesives adapted for sizing of cellulose fibre products f manufacture of the adhesive. The clay mix is made by mixing together 100 parts of Engsuch as paper, cotton 'or linen fabrics.

The term size is understood to include" so-called enginesize, surface size and also surface coating size, 1. e., the adhes ve (size) used to bind pigment to the surface of the paper in that-manufacture of coated paper.

By i ment I mean any material other k than tlie adhesive embodying olea'ginoils seed flour, which material is bound to the cellulose fibre 1pniduct includinlg such materials as. cla *ao in whitinb anc fixe, and the-like as halt, mmeral and fatt olls and rosin.

r est w 1c is'used to evaluate the adhesive strength of a size when used in conjunction with a pigment in the manufacture of coated papers, for instance, is the so-called sealing wax test. This test consists of determining the amount or proportion of fibre pulled from the paper when a piece of soft sealing wax is pressed against the surface, allowed to harden and then quickly removed. The test is made in comparison between a standard piece of coated paper and the sampleto be tested. 1 It is of'very material advantage to be able to give to each sample a numerical value. This is accomplished b v preparing a series of standards by making sealing wax tests of.

coated paper containing varying amounts or proportions of adhesive or size so that the results range from very poor to practically perfect. For instance, a paper so poorly coata ed, or the coating of which contains so poor an adhesive that the coating is completely .removed wherever touched by the sealing wax, without disturbance of the fibres of the cellulose fibre product, or paper, would he s given a value of zero. On the other hand, a coating so perfect or containing an adhesive with it not only the coating, fibre and paper itself beneath the coating amount ture is further agitated and then heated on Reference of such remarkable strength that the sealing wax when removed from the aper pulled ut also the wherever same was touched by the sealing wax, would be given a value of 100. It is necessary furthermore, in givin such numerical values to results obtaine to carefully control. all of the conditions under which the test is made. For instance, sealing wax having a constant melting point must be used, it must be heated to the same temperature be fore being applied to the paper in each instance, it must be applied to the paper with the same amount of pressure in each instance, allowed to remain for the same length of time and sharply removed in the same manner.

- Examiner Results given in these tests are the averages i of large numbers of results obtained in order that personal errors may be so far as possible eliminated.

In illustration of a cellulose fibre product embodying an oleaginous seed flour adhesive we may coat paper with English coating clay and use soya bean flour, as representative oleaginous seed flour contalnmg material, in the mixing together in a suitable mixing device 1.00 parts of soya bean flour, 500 parts of water, 6 arts of caustic soda and furfura1 in om 1 part to 20 parts. The mixa water bath to 150"F. and then cooled. The clay mix and adhesive mix are then mixed in suitable proportions and are ready for application of the paper. p

The test results given below are in exemplification of the material benefits to be derived as the result of my discovery using the same procedure as to methods of tests, formula for clay mix, adhesive mix, coating mix, etc., with the exception that the proportion of furfural added was varied as follows L-1 no furfural added to adhesive mix L-2 furfural was added in tllBPIOPOItlODS The remarkable increase in strength due to the embodiment of furfural is apparent.

It will be understood from the above that the adhesive or glueconsists of ingredients,

a part of which may be mixed together dry and form what, is called the dryEmix materials. These materials, thoroughly mixed comprises adding furfural to oleaginous seed flour containing material dispensed in an alkaline medium.

2. The method of making adhesives which comprises adding furfural to oleaginous seed flour and casein containing material dispersed in an alkaline medium.

3. The method of making adhesives which comprises adding furfural to soya bean flour containing material dispersed in an alkaline medium.

4. The method of making adhesives which I comprises adding furfural to soya bean flour -and casein containing material dispersed in an alkaline medium.

5. In the manufacture of an adhesive embodying oleaginous seed flour dispersed in an alkaline medium the step of adding thereto furfural.

6. In the manufacture of an adhesive embodying oleaginous seed flour and casein dispersed in an alkaline medium the step of adding thereto furfural.

7 In the manufacture of an adhesive embodying soya bean flour dispersed in an alkaline medium the step of adding thereto furfural.

8. In the manufacture of an adhesive embodying soya bean flour and casein dispersed in an alkaline medium the step of adding thereto furfural.

9. An adhesive which embodies the reaction products of oleaginous seed flour containing material dispersed in an alkaline medium and furfuralL 10. An adhesive which embodies the reaction products of oleaginous seed flour and casein containing material dispersed in an alkaline medium and furfural. I

11. An adhesive which embodies the reaction products of soya bean flour containing material dispersed in an alkaline medium and furfural.

12. Aniadhesive which embodies the reaction products of soya bean flour and casein containing material dispersed in an alkaline medium and furfural.

In witness whereof, I hereunto subscribe my namethis 18th day of January, 1929.

HARRY P. BANKS.

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